CN109652646A - A kind of method of nickel, cobalt, magnesium, silicon in the high magnesium silicon lateritic nickel ore of synthetical recovery - Google Patents
A kind of method of nickel, cobalt, magnesium, silicon in the high magnesium silicon lateritic nickel ore of synthetical recovery Download PDFInfo
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- CN109652646A CN109652646A CN201811560804.1A CN201811560804A CN109652646A CN 109652646 A CN109652646 A CN 109652646A CN 201811560804 A CN201811560804 A CN 201811560804A CN 109652646 A CN109652646 A CN 109652646A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 213
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 107
- 239000010941 cobalt Substances 0.000 title claims abstract description 44
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 44
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 43
- MKPXGEVFQSIKGE-UHFFFAOYSA-N [Mg].[Si] Chemical compound [Mg].[Si] MKPXGEVFQSIKGE-UHFFFAOYSA-N 0.000 title claims abstract description 30
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 22
- 239000011777 magnesium Substances 0.000 title claims abstract description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000011084 recovery Methods 0.000 title claims abstract description 20
- 239000010703 silicon Substances 0.000 title claims abstract description 20
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000007788 liquid Substances 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000002386 leaching Methods 0.000 claims abstract description 21
- 238000000605 extraction Methods 0.000 claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012530 fluid Substances 0.000 claims abstract description 12
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000012153 distilled water Substances 0.000 claims abstract description 11
- 239000006229 carbon black Substances 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000005868 electrolysis reaction Methods 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 15
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 10
- 239000003792 electrolyte Substances 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 10
- 239000002699 waste material Substances 0.000 claims description 10
- 241000080590 Niso Species 0.000 claims description 9
- 238000005516 engineering process Methods 0.000 claims description 9
- 239000000395 magnesium oxide Substances 0.000 claims description 9
- 239000012074 organic phase Substances 0.000 claims description 8
- 239000004567 concrete Substances 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 6
- 239000001117 sulphuric acid Substances 0.000 claims description 6
- 235000011149 sulphuric acid Nutrition 0.000 claims description 6
- 229910052681 coesite Inorganic materials 0.000 claims description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims description 5
- 239000012071 phase Substances 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229910052682 stishovite Inorganic materials 0.000 claims description 5
- 229910052905 tridymite Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 238000003723 Smelting Methods 0.000 abstract description 10
- 230000001681 protective effect Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 15
- 239000007789 gas Substances 0.000 description 12
- 239000002253 acid Substances 0.000 description 10
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 7
- 239000005864 Sulphur Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910052928 kieserite Inorganic materials 0.000 description 4
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 4
- 235000019341 magnesium sulphate Nutrition 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 125000004122 cyclic group Chemical group 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 229910001710 laterite Inorganic materials 0.000 description 3
- 239000011504 laterite Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- CNJLMVZFWLNOEP-UHFFFAOYSA-N 4,7,7-trimethylbicyclo[4.1.0]heptan-5-one Chemical compound O=C1C(C)CCC2C(C)(C)C12 CNJLMVZFWLNOEP-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910017709 Ni Co Inorganic materials 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000013601 eggs Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 210000004709 eyebrow Anatomy 0.000 description 1
- 210000000720 eyelash Anatomy 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3844—Phosphonic acid, e.g. H2P(O)(OH)2
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/06—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
- C25C1/08—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Life Sciences & Earth Sciences (AREA)
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- Geochemistry & Mineralogy (AREA)
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Abstract
A kind of method that the present invention discloses nickel, cobalt, magnesium, silicon in the high magnesium silicon lateritic nickel ore of synthetical recovery, high magnesium silicon lateritic nickel ore carry out ball milling, and it is (4-8) that miberal powder, which consolidate mass ratio according to liquid: 1 is added in sulfuric acid after leaching and filters；White carbon black is prepared in drying after leached mud is washed with distilled water, is filtered, and leachate is heated in autoclave, then high-pressure filteration, obtains filter residue and filtered fluid；In molar ratio it is 1:(1-1.5 by filter residue and carbon) it calcines at high temperature after mixing, obtain MgO and SO2, CO mixed gas, mixed gas enters process for preparing sulfuric acid；Filtered fluid is subjected to extraction back extraction and respectively obtains NiSO4And CoSO4Solution；By NiSO4Solution and CoSO4Solution is electrolysed to obtain nickel and cobalt respectively；Nickel, cobalt, magnesium, silicon components in synthetical recovery of the present invention lateritic nickel ore, improve the comprehensive utilization ratio of lateritic nickel ore, realize the high efficiency of smelting laterite-nickel ores technique, low consumption, low cost, environmentally protective.
Description
Technical field
The present invention relates to the methods of nickel, cobalt, magnesium, silicon in a kind of high magnesium silicon lateritic nickel ore of synthetical recovery, belong to non-ferrous metal
Field of metallurgy.
Technical background
Since mid-term the 1980s, metallic nickel is widely used in every field, such as: nickel steel and iron industry,
Magnetic industry, military affairs, non-ferrous metal, noble metal, specific alloy, hydrogen storage material, Special Nickel Powder, novel painting nickel composite material, electricity
The applicating and exploitation of pond, health care and nickel sulfate etc. is very noticeable.Nickel is as a kind of important strategy metal, tool
There are good mechanical strength, ductility and chemical stability, is the industry metal indispensable with mankind's modern civilization is developed,
There is extremely important status in the national economic development.
Magnesia is also wide in addition to being used for refractory material and smelting magnesium as a kind of important inorganic chemical product
It is general to be applied to the numerous areas such as paper pulp, construction material, fertilizer, rubber, plastics and binder.
White carbon black, that is, hydrated SiO 2 is a kind of unformed white powder, have large specific surface area, high surface activity with
And the characteristics such as superior stability, reinforcing, thickening property, extinction, thus it is widely used in electronics, food, medicine, chemical industry
Equal fields.
Lateritic nickel ore be usually by the nickeliferous olivine of the torrid zone and subtropical zone by long-time weathering leaching consider it is rotten and
The mineral of the multiple elements such as iron content, aluminium, oxygen, silicon, magnesium, nickel, the cobalt of formation are distributed mainly on the circum pacific torrid zone-subtropical zone
Area.Nickel resources are relatively abundanter on the earth, and current explored continental rise nickel resources are about 2.3 hundred million t, and wherein lateritic nickel ore accounts for
72.2%, average grade 1.28%.China is nickel resources than one of more rich country, and having verified nickel resources is about 7,850,000 t,
Gansu, Xinjiang, Yunnan, Jilin, Hubei, Sichuan, Shaanxi, eight, Qinghai provinces and regions are mainly distributed on, wherein Yunnan laterite nickel minerals is
52.6 ten thousand t account for the 69% of China's lateritic nickel ore resource.Since the nickel sulfide ore resource in the world for exploitation is fewer and fewer, with
The high speed development of world economy, nickel increase in demand, price raise up, and the dressing and smelting process research of low-grade laterite nickel ore has been compeled in eyebrow
Eyelash.
About the development and utilization of low-grade laterite nickel ore, scholar both domestic and external is just carried out since the sixties in last century
A large amount of research work proposes numerous smelting processes, rotary kiln drying prereduction-electric furnace smelting process including thermal process
(RKEF), sintering-blast furnace sulfiding smelting method, reduction roasting-magnetic method；Reduction roasting-ammonia leaching method (the Caron of wet processing
Process), pressurized acid leaching method, the normal pressure acid-hatching of young eggs, dump leaching method, alkali soaking technology etc., part of smelting process realizes industrialization and answers
With, but all smelting processes both in lateritic nickel ore nickel, cobalt extraction come what is carried out, smelting process does not utilize mine
Magnesium in object generates a large amount of waste residue, waste liquid, is unfavorable for environmental protection, especially pressurized acid leaching and normal pressure acid leaching process, generates big
The magnesium sulfate waste liquid of amount, not only waste liquid is difficult to handle, while consuming a large amount of sulfuric acid, it is also difficult to realize the synthetical recovery of lateritic nickel ore
It utilizes.
Summary of the invention
Work as existing shortcoming for above-mentioned technique, the present invention provides in a kind of high magnesium silicon lateritic nickel ore of synthetical recovery
The method of nickel, cobalt, magnesium, silicon, the present invention provides a kind of wet method combined technology of pyrogenic process-, acid leaching residue prepares white carbon black, acid
Leaching-high-pressure filteration-calcining prepares high-purity magnesium oxide, sour leaching-extraction back extraction-electrolytic preparation nickel product, cobalt product.
The invention is realized by the following technical scheme:
A kind of method of nickel, cobalt, magnesium, silicon in the high magnesium silicon lateritic nickel ore of synthetical recovery, the specific steps are as follows:
(1) high magnesium silicon lateritic nickel ore is subjected to ball milling, sieved with 100 mesh sieve, obtain lateritic nickel ore powder；
(2) it is (4-8) that the miberal powder that step (1) obtains, which consolidates mass ratio according to liquid: 1 ratio, which is added in sulfuric acid, leaches 4-6h, mistake
Filter obtains leached mud and leachate；
(3) leached mud that step (2) obtains be washed with distilled water, filter after dry, according to solid-liquid mass ratio be 1:(20-40)
Ratio is mixed with the NaOH solution that mass fraction is 5-25%, and mixed liquor boils and stir 0.5-2h, and 2-3 times of body is added after cooling
Long-pending water is (1.4-1.7) according still further to volume ratio: the NaCl solution that 1 ratio and concentration is 80g/L mixes, and is heated to 60-80
DEG C, pH value is adjusted to 7.0, and ageing 30min or more is rear to be filtered, and filter residue is rinsed 5-7 times and taken out repeatedly with 50-70 DEG C of hot distilled water
After filter, 120-160 DEG C of drying obtains white carbon black；
(4) leachate that step (2) obtains heats in autoclave, and then high-pressure filteration, obtains filter residue and filtered fluid；
(5) filter residue and carbon that step (4) obtains are (8-12) according to mass ratio: 1 ratio after mixing, carries out at high temperature
Calcining, obtains MgO and SO2, CO mixed gas, mixed gas enters Sulphuric acid process；
(6) filtered fluid that step (4) obtains carries out extraction back extraction and respectively obtains NiSO4Solution and CoSO4Solution；
(7) NiSO that step (6) obtains4Solution and CoSO4Solution is electrolysed to obtain nickel and cobalt respectively.
Each material mass degree in the high magnesium silicon lateritic nickel ore of step (1) are as follows: Ni1.5-3.0%；Co0.02-0.1%；
MgO15-35%；SiO230-50%；Fe10-25%；CrO3%；Surplus is water and inevitable impurity.
The concentration of step (2) sulfuric acid is 360g/L ~ 1800g/L.
Temperature in step (4) autoclave is 140 ~ 220 DEG C, pressure 1.0-4.5MPa；The pressure of high-pressure filteration is
1.0-4.5MPa。
Step (5) calcining is 800-1600 DEG C of heat preservation 2-4h under vacuum conditions.
Leaching liquid is used as in sulfuric acid return step (2) made from step (5) Sulphuric acid process.
The concrete technology of step (6) extraction back extraction is: carrying out pre-extracted, raffinate to impurity therein using P204 first
Ni, Co are separated using P507 again, nickel is with NiSO4Form is present in water phase, organic phase then use concentration for 150g/L ~
350g/L sulfuric acid is stripped to obtain CoSO4Solution.
The concrete technology of step (7) electrolysis is: by NiSO4The pH value of solution is adjusted to 4.5-5.5 as electrolyte, with nickel
Electrode is as cathode, and lead electrode is as anode, in 50 DEG C, tank voltage 3-4V, current density 200-300A/m2Under conditions of
Electrolysis obtains nickel；By CoSO4The pH value of solution is adjusted to 4.5-5.5 as electrolyte, and using nickel starting sheet as cathode, thick cobalt is electric
Pole is as anode, in 50 DEG C, tank voltage 2-4V, current density 300-500A/m2Under conditions of electrolysis obtain cobalt.
Leaching liquid is used as in step (7) electrolysis waste solution return step (2).
The beneficial effects of the present invention are:
(1) it is directed to the problem of lateritic nickel ore comprehensive reutilization difficulty, acidleach-high pressure-temperature crystallization-high-pressure filteration-is proposed and adds
Carbon calcining, acidleach-high-pressure filteration-extraction back extraction-electrolysis technical solution, realize the sulphur of high magnesium silicon lateritic nickel ore acid leaching process
Acid circulation is a kind of high efficiency, low consumption, low cost, environmentally protective smelting process.
(2) feature low using magnesium sulfate high-temperature digestion degree, is warming up to 140-220 DEG C for solution in autoclave, makes molten
Most of magnesium sulfate in liquid crystallizes into MgSO4·H2O, and in order to prevent magnesium sulfate return it is molten, by the way of high-pressure filteration into
Row is separated by solid-liquid separation.
(3) obtained MgSO is crystallized4·H2O adds carbon to calcine by high temperature, available MgO and SO2, CO mixed gas,
Middle SO2It is sent into acid making system extracting sulfuric acid, and sulfuric acid is returned into leaching step in sulfuric acid, by NiSO4Solution and CoSO4Solution
Electrolysis waste solution after electrolysis returns to leaching step in sulfuric acid, and sulfuric acid is enable to recycle.
Specific embodiment
Combined with specific embodiments below, the invention will be further described.
Embodiment 1
A kind of method of nickel, cobalt, magnesium, silicon in the high magnesium silicon lateritic nickel ore of synthetical recovery, the specific steps are as follows:
(1) high magnesium silicon lateritic nickel ore is subjected to ball milling, sieved with 100 mesh sieve, obtain lateritic nickel ore powder, each object in high magnesium silicon lateritic nickel ore
Matter mass percentage content are as follows: Ni2.0%；Co0.05%；MgO25%；SiO240%；Fe10%；CrO3%；Surplus is water and can not keep away
Exempt from impurity；
(2) it is that be added to concentration be that 6h, mistake are leached in 360g/L sulfuric acid to 4:1 that the miberal powder that step (1) obtains, which consolidates mass ratio according to liquid,
Filter obtains leached mud and leachate；
(3) leached mud that step (2) obtains be washed with distilled water, filter after dry, according to solid-liquid mass ratio be 1:20 ratio
The NaOH solution for being 5% with mass fraction mixes, and mixed liquor boils and stir 0.5h, and 2 times of volumes of mixed liquor are added after cooling
Water, according still further to volume ratio be 1.7:1 ratio and concentration be 80g/L NaCl solution mix after, 80 DEG C are heated to, using dilute sulphur
Solution ph is adjusted to 7.0 by acid, is filtered after being aged 30min, and filter residue rinses 5 times with 50 DEG C of hot distilled water repeatedly and filters,
Then 5 hours are kept the temperature at 120 DEG C to dry, obtains white carbon black；
(4) leachate that step (2) obtains heats in autoclave, and the temperature in autoclave is 140 DEG C, pressure 4.5MPa,
Then it is 4.5MPa high-pressure filteration in pressure, obtains MgSO4·H2O crystal filter residue and filtered fluid；
(5) MgSO that step (4) obtains4·H2O crystal filter residue and carbon according to the ratio that mass ratio is 8:1 after mixing,
Under vacuum condition, 1600 DEG C of heat preservation 2h are calcined, and obtain MgO and SO2, CO mixed gas, mixed gas enters Sulphuric acid
Technique obtains sulfuric acid, is used as leaching liquid in sulfuric acid return step (2), and a small amount of CO is oxidized to CO in mixed gas2Emptying；
(6) filtered fluid that step (4) obtains uses P204 to carry out pre-extracted to impurity therein first, and raffinate uses P507 again
Separation of nickel and cobalt is carried out, 90% or more cobalt enters in organic phase after this operation, and nickel then stays in and obtains NiSO in water phase4It is molten
Then liquid uses concentration to carry out back extraction to organic phase for the sulfuric acid of 150g/L and handles to obtain CoSO4Solution；
(7) NiSO that step (6) obtains4Solution and CoSO4Solution is electrolysed to obtain nickel and cobalt, the concrete technology of electrolysis respectively
It is: by NiSO4Solution adjusts pH value to 4.5 as electrolyte using dilute sulfuric acid, and using nickel electrode as cathode, lead electrode is as sun
Pole, in 50 DEG C, voltage 3V, current density 200A/m2Under conditions of be electrolysed, obtain nickel in cathode；By CoSO4Solution
PH value is adjusted using dilute sulfuric acid and is used as electrolyte to 4.5, using nickel starting sheet as cathode, thick cobalt electrode as anode, 50 DEG C,
Tank voltage is 2V, current density 300A/m2Under conditions of be electrolysed, obtain cobalt in cathode；Electrolysis waste solution return step (2)
It is middle to be used as leaching liquid.
The cyclic utilization rate of element sulphur is 80% in the present embodiment.
Each stage product purity of the present embodiment is shown in Table 1:
Each stage product purity of table 1
。
Embodiment 2
A kind of method of nickel, cobalt, magnesium, silicon in the high magnesium silicon lateritic nickel ore of synthetical recovery, the specific steps are as follows:
(1) high magnesium silicon lateritic nickel ore is subjected to ball milling, sieved with 100 mesh sieve, obtain lateritic nickel ore powder, each object in high magnesium silicon lateritic nickel ore
Matter mass percentage content are as follows: Ni3.0%；Co0.1%；MgO35%；SiO230%；Fe25%；CrO3%；Surplus is water and can not keep away
Exempt from impurity；
(2) it is that be added to concentration be that 5h, mistake are leached in 760g/L sulfuric acid to 6:1 that the miberal powder that step (1) obtains, which consolidates mass ratio according to liquid,
Filter obtains leached mud and leachate；
(3) leached mud that step (2) obtains be washed with distilled water, filter after dry, according to solid-liquid mass ratio be 1:30 ratio
The NaOH solution for being 15% with mass fraction mixes, and mixed liquor boils and stir 1h, and 2.5 times of volumes of mixed liquor are added after cooling
Water, according still further to volume ratio be 1.5:1 ratio and concentration be 80g/L NaCl solution mix after, 60 DEG C are heated to, using dilute sulphur
Solution ph is adjusted to 7.0 by acid, is filtered after being aged 60min, and filter residue rinses 6 times with 70 DEG C of hot distilled water repeatedly and filters,
Then 3 hours are kept the temperature at 150 DEG C to dry, obtains white carbon black；
(4) leachate that step (2) obtains heats in autoclave, and the temperature in autoclave is 180 DEG C, pressure 2MPa, so
It is afterwards 2MPa high-pressure filteration in pressure, obtains MgSO4·H2O crystal filter residue and filtered fluid；
(5) MgSO that step (4) obtains4·H2O crystal filter residue and carbon according to the ratio that mass ratio is 12:1 after mixing,
Under vacuum condition, 800 DEG C of heat preservation 4h are calcined, and obtain MgO and SO2, CO mixed gas, mixed gas enters Sulphuric acid work
Skill obtains sulfuric acid, is used as leaching liquid in sulfuric acid return step (2), and a small amount of CO is oxidized to CO in mixed gas2Emptying；
(6) filtered fluid that step (4) obtains uses P204 to carry out pre-extracted to impurity therein first, and raffinate uses P507 again
Separation of nickel and cobalt is carried out, 95% or more cobalt enters in organic phase after this operation, and nickel then stays in and obtains NiSO in water phase4It is molten
Then liquid uses concentration to carry out back extraction to organic phase for the sulfuric acid of 200g/L and handles to obtain CoSO4Solution；
(7) NiSO that step (6) obtains4Solution and CoSO4Solution is electrolysed to obtain nickel and cobalt, the concrete technology of electrolysis respectively
It is: by NiSO4Solution adjusts pH value to 5 as electrolyte using dilute dilute sulfuric acid, and using nickel electrode as cathode, lead electrode is as sun
Pole, in 50 DEG C, voltage 3.5V, current density 250A/m2Under conditions of be electrolysed, obtain nickel in cathode；By CoSO4It is molten
Liquid adjusts pH value using dilute sulfuric acid and is used as electrolyte to 5, using nickel starting sheet as cathode, thick cobalt electrode as anode, 50 DEG C,
Tank voltage is 3V, current density 400A/m2Under conditions of be electrolysed, obtain cobalt in cathode；Electrolysis waste solution return step (2)
It is middle to be used as leaching liquid.
The cyclic utilization rate of element sulphur is 90% in the present embodiment.
Each stage product purity of the present embodiment is shown in Table 2:
Each stage product purity of table 2
。
Embodiment 3
A kind of method of nickel, cobalt, magnesium, silicon in the high magnesium silicon lateritic nickel ore of synthetical recovery, the specific steps are as follows:
(1) high magnesium silicon lateritic nickel ore is subjected to ball milling, sieved with 100 mesh sieve, obtain lateritic nickel ore powder, each object in high magnesium silicon lateritic nickel ore
Matter mass percentage content are as follows: Ni1.5%；Co0.02%；MgO15%；SiO250%；Fe15%；CrO3%；Surplus is water and can not keep away
Exempt from impurity；
(2) it is that be added to concentration be that 4h, mistake are leached in 1800g/L sulfuric acid to 8:1 that the miberal powder that step (1) obtains, which consolidates mass ratio according to liquid,
Filter obtains leached mud and leachate；
(3) leached mud that step (2) obtains be washed with distilled water, filter after dry, according to solid-liquid mass ratio be 1:40 ratio
The NaOH solution for being 25% with mass fraction mixes, and mixed liquor boils and stir 2h, and the water of 3 times of volumes of mixed liquor is added after cooling,
According still further to volume ratio be 1.4:1 ratio and concentration be 80g/L NaCl solution mix after, 70 DEG C are heated to, using dilute sulfuric acid
Solution ph is adjusted to 7.0, is filtered after being aged 50min, filter residue rinses 7 times with 60 DEG C of hot distilled water repeatedly and filters, so
2 hours are kept the temperature at 160 DEG C afterwards to dry, and obtain white carbon black；
(4) leachate that step (2) obtains heats in autoclave, and the temperature in autoclave is 220 DEG C, pressure 1MPa, so
It is afterwards 1MPa high-pressure filteration in pressure, obtains MgSO4·H2O crystal filter residue and filtered fluid；
(5) MgSO that step (4) obtains4·H2O crystal filter residue and carbon according to the ratio that mass ratio is 10:1 after mixing,
Under conditions of vacuum, 1000 DEG C of heat preservation 3h are calcined, and obtain MgO and SO2, CO mixed gas, mixed gas enters sulphur processed
Sour technique obtains sulfuric acid, is used as leaching liquid in sulfuric acid return step (2), and a small amount of CO is oxidized to CO in mixed gas2Emptying；
(6) filtered fluid that step (4) obtains uses P204 to carry out pre-extracted to impurity therein first, and raffinate uses P507 again
Separation of nickel and cobalt is carried out, 97% or more cobalt enters in organic phase after this operation, and nickel then stays in and obtains NiSO in water phase4It is molten
Then liquid uses concentration to carry out back extraction to organic phase for the sulfuric acid of 350g/L and handles to obtain CoSO4Solution；
(7) NiSO that step (6) obtains4Solution and CoSO4Solution is electrolysed to obtain nickel and cobalt, the concrete technology of electrolysis respectively
It is: by NiSO4Solution adjusts pH value to 5.5 as electrolyte using dilute sulfuric acid, and using nickel electrode as cathode, lead electrode is as sun
Pole, in 50 DEG C, voltage 4V, current density 300A/m2Under conditions of be electrolysed, obtain nickel in cathode；By CoSO4Solution
PH value is adjusted using dilute sulfuric acid and is used as electrolyte to 5.5, using nickel starting sheet as cathode, thick cobalt electrode as anode, 50 DEG C,
Tank voltage is 4V, current density 500A/m2Under conditions of be electrolysed, obtain cobalt in cathode；Electrolysis waste solution return step (2)
It is middle to be used as leaching liquid.
The cyclic utilization rate of element sulphur is 88% in the present embodiment.
Each stage product purity of the present embodiment is shown in Table 3:
Each stage product purity of table 3
| Substance | White carbon black | MgO | Ni | Co |
| Purity | > 99 | > 99 | > 99.99 | > 99.99 |
A specific embodiment of the invention is described in detail above, but present invention is not limited to the embodiments described above,
In the knowledge that those skilled in the art are grasped, various changes can also be carried out without departing from the purpose of the present invention
Change.
Claims (9)
1. a kind of method of nickel, cobalt, magnesium, silicon in high magnesium silicon lateritic nickel ore of synthetical recovery, which is characterized in that specific step is as follows:
(1) high magnesium silicon lateritic nickel ore is subjected to ball milling, sieved with 100 mesh sieve, obtain lateritic nickel ore powder；
(2) it is (4-8) that the miberal powder that step (1) obtains, which consolidates mass ratio according to liquid: 1 ratio, which is added in sulfuric acid, leaches 4-6h, mistake
Filter obtains leached mud and leachate；
(3) leached mud that step (2) obtains be washed with distilled water, filter after dry, according to solid-liquid mass ratio be 1:(20-40)
Ratio is mixed with the NaOH solution that mass fraction is 5-25%, and mixed liquor boils and stir 0.5-2h, and 2-3 times of body is added after cooling
Long-pending water is (1.4-1.7) according still further to volume ratio: the NaCl solution that 1 ratio and concentration is 80g/L mixes, and is heated to 60-80
DEG C, pH value is adjusted to 7.0, and ageing 30min or more is rear to be filtered, and filter residue is rinsed 5-7 times and taken out repeatedly with 50-70 DEG C of hot distilled water
After filter, 120-160 DEG C of drying obtains white carbon black；
(4) leachate that step (2) obtains heats in autoclave, and then high-pressure filteration, obtains filter residue and filtered fluid；
(5) filter residue and carbon that step (4) obtains are (8-12) according to mass ratio: 1 ratio after mixing, carries out at high temperature
Calcining, obtains MgO and SO2, CO mixed gas, mixed gas enters Sulphuric acid process；
(6) filtered fluid that step (4) obtains carries out extraction back extraction and respectively obtains NiSO4Solution and CoSO4Solution；
(7) NiSO that step (6) obtains4Solution and CoSO4Solution is electrolysed to obtain nickel and cobalt respectively.
2. according to claim 1 in the high magnesium silicon lateritic nickel ore of synthetical recovery nickel, cobalt, magnesium, silicon method, which is characterized in that
Each material mass degree in the high magnesium silicon lateritic nickel ore of step (1) are as follows: Ni1.5-3.0%；Co0.02-0.1%；MgO15-
35%；SiO230-50%；Fe10-25%；CrO3%；Surplus is water and inevitable impurity.
3. according to claim 1 in the high magnesium silicon lateritic nickel ore of synthetical recovery nickel, cobalt, magnesium, silicon method, which is characterized in that
The concentration of step (2) sulfuric acid is 360g/L ~ 1800g/L.
4. according to claim 1 in the high magnesium silicon lateritic nickel ore of synthetical recovery nickel, cobalt, magnesium, silicon method, which is characterized in that
Temperature in step (4) autoclave is 140 ~ 220 DEG C, pressure 1.0-4.5MPa；The pressure of high-pressure filteration is 1.0-4.5MPa.
5. according to claim 1 in the high magnesium silicon lateritic nickel ore of synthetical recovery nickel, cobalt, magnesium, silicon method, which is characterized in that
Step (5) calcining is 800-1600 DEG C of heat preservation 2-4h under vacuum conditions.
6. according to claim 1 in the high magnesium silicon lateritic nickel ore of synthetical recovery nickel, cobalt, magnesium, silicon method, which is characterized in that
Leaching liquid is used as in sulfuric acid return step (2) made from step (5) Sulphuric acid process.
7. according to claim 1 in the high magnesium silicon lateritic nickel ore of synthetical recovery nickel, cobalt, magnesium, silicon method, which is characterized in that
The concrete technology of step (6) extraction back extraction is: carrying out pre-extracted to impurity therein using P204 first, raffinate uses again
P507 separates Ni, Co, and NiSO is obtained in water phase4, organic phase uses concentration to be stripped for 150g/L ~ 350g/L sulfuric acid
Obtain CoSO4Solution.
8. according to claim 1 in the high magnesium silicon lateritic nickel ore of synthetical recovery nickel, cobalt, magnesium, silicon method, which is characterized in that
The concrete technology of step (7) electrolysis is: by NiSO4The pH value of solution is adjusted to 4.5-5.5 as electrolyte, using nickel electrode as
Cathode, lead electrode is as anode, in 50 DEG C, tank voltage 3-4V, current density 200-300A/m2Under conditions of be electrolysed and obtain
Nickel；By CoSO4The pH value of solution is adjusted to 4.5-5.5 as electrolyte, and using nickel starting sheet as cathode, thick cobalt electrode is as sun
Pole, in 50 DEG C, tank voltage 2-4V, current density 300-500A/m2Under conditions of electrolysis obtain cobalt.
9. according to claim 1 in the high magnesium silicon lateritic nickel ore of synthetical recovery nickel, cobalt, magnesium, silicon method, which is characterized in that
Leaching liquid is used as in step (7) electrolysis waste solution return step (2).
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